Faculty Publications
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Item A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective demasking property of 2-mercapto propionyl glycine (MPGH2) towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is back titrated at pH 5-5.5 (acetic acid-acetate buffer) with standard zinc sulphate solution using xylenol orange as indicator. An excess of a 0.2% aqueous solution of MPGH2 is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard zinc sulphate solution as before. Reproducible and accurate results are obtained in the concentration range 2-22 mg of palladium with relative error of ±0.36% and coefficient of variation (n=6) not exceeding 0.31%. The effect of diverse ions are studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.(Complexometric determination of palladium(II) using 2-mercapto propionyl glycine as demasking agent) Shetty, P.; Nityananda Shetty, A.N.; Gadag, R.V.2002Item A simple, rapid, selective and sensitive spectrophotometric method for the determination of palladium is proposed using piperonal thiosemicarbazone (PATS) as a reagent. The reagent forms a 1:2 complex (Pd:Reagent) with palladium. The yellow complex is soluble in 32-40% ethanol and has an absorption maximum at 363 nm. Beer's law is obeyed upto 3.85 ppm of palladium and the optimum concentration range is 0.5-2.45 ppm of Pd. The molar absorptivity and Sandell's sensitivity are 3. 80 x 104 dm3 mol-1 cm -1 and 2.8 x 10-3 ?g cm-2, respectively. The experimental conditions for complete colour development and the interference from various ions are investigated. The method is used for the determination of palladium in its complexes and synthetic mixtures.(Spectrophotometric determination of palladium(II) using piperonal thiosemicarbazone) Shetty, P.; Nityananda Shetty, A.N.; Gadag, R.V.2003Item A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of thioacetamide towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is back titrated at pH 5-5.5(acetic acid-sodium acetate buffer) with standard lead nitrate solution using xylenol orange as indicator. An excess of a 0.5% aqueous solution of thioacetamide is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard lead nitrate solution as before. Reproducible and accurate results are obtained in the concentration range 0.5mg-17.80mg of palladium with relative error of ±0.16% and coefficient of variation not exceeding 0.26%. The effect of diverse ions is studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.(Complexometric determination of palladium(II) using thioacetamide as a selective masking agent) Parameshwara, P.; Karthikeyan, J.; Nityananda Shetty, A.N.; Shetty, P.2006Item 4-(N,N-diethylamino) benzaldehyde thiosemicarbazone in the spectrophotometric determination of palladium(2007) Parameshwara, P.; Karthikeyan, J.; Nityananda Shetty, A.N.; Shetty, P.4-(N,N-diethylamino)benzaldehyde thiosemicarbazone(DEABT) is proposed as a sensitive and selective analytical reagent for the spectrophotometric determination of palladium(II). The reagent reacts with palladium (II) in a potassium hydrogen phthalate-hydrochloric acid buffer of pH 3.0, to form a yellow complex. Beer's law is obeyed in the concentration range up to 3.60 ?gmL-1. The optimum concentration range for minimum photometric error as determined by Ringbom plot method is 0.36-3.24 ?g mL-1. The yellow Pd(II)-DEABT complex shows a maximum absorbance at 408 nm, with molar absorptivity of 3.33 × 104 dm3 mol-1 cm-1 and Sandell's sensitivity of the complex from Beer's data, for D=0.001, is 0.0032 ?g cm-2. The composition of the Pd(II)-DEABT complex is found to be 1:2 (M:L). The interference of various cations and anions in the method were studied. The proposed method was successfully used for the determination of Pd(II) in alloys, catalysts, complexes and model mixtures with a fair degree of accuracy.Item Analytical properties of p-[N,N-bis(2-chloroethyl)amino]benzaldehyde thiosemicarbazone: Spectrophotometric determination of palladium(II) in alloys, catalysts, and complexes(2011) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.p-[N,N-bis(2-chloroethyl)amino]benzaldehyde thiosemicarbazone (CEABT) is proposed as a new, sensitive, and selective analytical reagent for the spectrophotometric determination of palladium(II). The reagent reacts with palladium(II) in the pH range 1-2 to form a yellow-colored complex. Beer's law is obeyed in the concentration range up to 2.64 ?g cm-3. The optimum concentration range for minimum photometric error as determined by Ringbom's plot method is 0.48-2.40 ?g cm-3. The yellowish Pd(II)-reagent complex shows a maximum absorbance at 395 nm, with molar absorptivity of 4.05 × 104 dm3 mol-1 cm-1 and Sandell's sensitivity of the complex from Beer's data, for D= 0.001, is 0.0026 ?g cm-2. The composition of the Pd(II)-CEABT reagent complex is found to be 1:2 (M-L). The interference of various cations and anions in the method were studied. The proposed method was successfully used for the determination of Pd(II) in alloys, catalysts, complexes, water samples, and synthetic alloy mixtures with a fair degree of accuracy. © 2010 Springer Science+Business Media B.V.Item Palladium complex in a room temperature ionic liquid: A convenient recyclable reagent for catalytic oxidation(Taylor and Francis Ltd., 2014) Dileep, R.; Badekai Ramachandra, B.; Suresha Kumara, T.H.S.Palladium (Pd)-catalyzed carbonylation of alcohols proceeds in ionic liquid (IL) media (1-ethyl-3-methylimidazolium hexafluorophosphate). Carbonylation of primary/secondary alcohols to aldehydes/ketones was greatly accelerated by the use of a Pd-based catalyst in the presence of NaOCl as an oxidant. The catalyst was more easier to recycle in the IL [Emim]PF6 with an equal-proportioned CH2Cl2 than in the single CH2Cl2 or IL. © 2014 The Author(s). Published by Taylor & Francis.Item Visible-light induced effective and sustainable remediation of nitro organics pollutants using Pd-doped ZnO nanocatalyst(Nature Research, 2024) Vikal, S.; Meena, S.; Gautam, Y.K.; Kumar, A.; Sethi, M.; Meena, S.; Gautam, D.; Singh, B.P.; Agarwal, P.C.; Meena, M.L.; Parewa, V.Nitroaromatic compounds represent a class of highly toxic pollutants discharged into aquatic environments by various industrial activities, posing significant threats to ecological integrity and human health due to their persistent and hazardous nature. In this study, Pd-doped ZnO nanoparticles were investigated as a potential solution for the degradation of nitro organics, offering heightened photocatalytic efficacy and prolonged stability. The synthesis of Pd-doped ZnO NPs was achieved via the hydrothermal method, with subsequent analysis through XRD spectra and XPS confirming successful Pd doping within the ZnO matrix. Characterization through FESEM and HRTEM unveiled the heterogeneous morphologies of both undoped and Pd-doped ZnO nanoparticles. Additionally, UV–vis and PL spectroscopy provided insights into the optical properties, chemical bonding, and defect structures of the synthesized Pd-doped ZnO NPs. Pd doping induces a redshift in ZnO’s absorption spectra, reducing the bandgap from 3.12 to 2.94 eV as Pd concentration rises from 0 to 0.2 wt.%. The photocatalytic degradation, following pseudo-first-order kinetics, achieved 90% nitrobenzene abatement (200 µg/L, pH 7) under visible light within 320 min with a catalyst loading of 16 µg/mL. The photocatalytic efficacy of 0.08 wt% Pd-doped ZnO (k = 0.058 min?1) exhibited a 25-fold enhancement compared to bare ZnO (k = 3.1 × 10–4 min-1). Subsequent quenching and ESR experiments identified hydroxyl radicals (OH•) as the predominant active species in the degradation mechanism. Mass spectrometry analysis unveiled potential breakdown intermediates, illuminating a plausible degradation pathway. The investigated Pd-doped ZnO nanoparticles demonstrated reusability for up to five successive treatment cycles, offering a sustainable solution to nitro organics contamination challenges. © The Author(s) 2024.